CN118198383A - Method for modifying surface of microporous layer of gas diffusion layer of fuel cell - Google Patents
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- 238000001652 electrophoretic deposition Methods 0.000 claims abstract description 31
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- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 18
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
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- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 16
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
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- 238000003756 stirring Methods 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
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- 229910021389 graphene Inorganic materials 0.000 claims description 4
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- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
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- 239000002270 dispersing agent Substances 0.000 claims description 2
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- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 12
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 12
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- 229910052684 Cerium Inorganic materials 0.000 abstract 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
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- 210000004027 cell Anatomy 0.000 description 17
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- 230000000052 comparative effect Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
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- 238000003487 electrochemical reaction Methods 0.000 description 3
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
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- 239000003456 ion exchange resin Substances 0.000 description 2
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- 150000003460 sulfonic acids Chemical class 0.000 description 2
- 239000004890 Hydrophobing Agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Abstract
The invention relates to the technical field of fuel cells, in particular to a method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, wherein the gas diffusion layer consists of a basal layer, a conventional microporous layer and a modified microporous layer. And immersing the modified microporous layer into an electrophoretic deposition liquid formed by mixing cerium salt, carbon powder and PTFE after conventional coating, drying and presintering processes to serve as a negative electrode for electrophoretic deposition, depositing a layer of metal cerium, carbon particles and PTFE coating on the surface of the conventional microporous layer, and then drying and sintering the porous layer to obtain a layer of hydrophobic microporous layer containing nano cerium oxide particles on the surface of the microporous layer. The gas diffusion layer with the surface modified can effectively capture HO free radicals generated in the reaction when the galvanic pile is in operation, prevent degradation of the proton exchange membrane caused by free radical attack, and improve the durability of the membrane electrode of the fuel cell.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell.
Background
Proton Exchange Membrane Fuel Cells (PEMFC) have been a clean and efficient battery system developed in the last century. The battery has the characteristics of simple structure, high power density, high energy conversion efficiency, low-temperature start, no pollution, light weight and the like. The main components of the PEMFC are a bipolar plate, a gas diffusion layer, a catalyst layer and a proton exchange membrane.
In PEMFC, the proton exchange membrane is positioned in the center of the membrane electrode, plays roles of isolating gas and conducting protons, and the ion exchange resin is positioned in the catalytic layer and coated on the surface of the catalyst, thus playing roles of conducting protons and bonding the catalyst. The proton exchange membrane and the ion exchange resin are usually perfluorinated sulfonic acid resin, and free radicals generated in the electrochemical reaction process attack key groups in the perfluorinated sulfonic acid resin, so that the resin and the membrane are degraded, and the service life of the PEMFC is reduced. Therefore, in view of the above-mentioned current situation, there is an urgent need to develop a means for effectively capturing free radicals generated in an electrochemical reaction to overcome the shortcomings in the current practical application.
The gas diffusion layers are positioned at two sides of the catalytic layer and play roles in gas conduction, electric conduction, drainage, heat conduction and preparation.
Disclosure of Invention
The present invention is directed to a method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, which solves the above-mentioned problems of the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for modifying the surface of microporous layer of gas diffusion layer of fuel cell is disclosed, which comprises the following steps:
step one: placing the carbon paper substrate in a hydrophobizing agent, taking out, removing surface floating liquid, drying, and then placing in a sintering furnace for sintering to obtain a hydrophobic substrate layer;
step two: preparing uniform and stable microporous layer slurry of the gas diffusion layer by fully stirring and mixing carbon powder, a hydrophobic agent, a solvent and an additive according to a certain proportion;
Step three: coating the prepared microporous layer slurry on the surface of the hydrophobic treated substrate layer in a doctor blade coating, spraying or screen printing mode, and drying to obtain a conventional microporous layer;
Step four: presintering the conventional microporous layer to obtain a gas diffusion layer with stable structure and slight hydrophobicity;
Step five: placing the slightly hydrophobic gas diffusion layer obtained in the step four into an electrophoretic deposition device for electrophoretic deposition, taking out the slightly hydrophobic gas diffusion layer, removing surface floating liquid, and drying to obtain a modified microporous layer;
step six: finally, the surface modified gas diffusion layer is obtained through high-temperature sintering.
Preferably, in the method for modifying the surface of the microporous layer of the gas diffusion layer of the fuel cell according to the first step, the substrate layer is carbon fiber paper or carbon fiber cloth, the hydrophobic substrate layer is obtained by soaking a hydrophobizing agent with a mass fraction of 5wt.% to 15wt.%, drying at 80 ℃ to 120 ℃ and sintering at 340 ℃ to 380 ℃, and after the hydrophobic treatment, the solid content of PTFE is controlled to be 5% to 15% of the mass of the original substrate layer, and the hydrophobizing agent is one or more of PTFE and PVDF.
Preferably, in the method for modifying a surface of a microporous layer of a gas diffusion layer of a fuel cell in the second step, the proportion of the microporous layer slurry is generally carbon powder: hydrophobing agent: solvent: additive = 1:0.1:20:0.01-1:1:5:0.1, the carbon powder is one or more of carbon black, acetylene black and carbon nano tubes, the solvent is one or more of water, ethanol, ethylene glycol, n-propanol and isopropanol, and the additive comprises a pore-forming agent, a dispersing agent, a thickening agent, a leveling agent and the like.
Preferably, in the method for modifying the surface of the microporous layer of the gas diffusion layer of the fuel cell according to the fourth step, the presintering temperature of the conventional microporous layer may be set to 180-320 ℃, and the presintering time may be set to 10-30min.
Preferably, the method for modifying the surface of the microporous layer of the gas diffusion layer of the fuel cell in the fifth step is characterized in that the electrophoretic deposition device is a two-electrode system device, the anode is a counter electrode, a stainless steel sheet is arranged, and the cathode is an electrophoretic deposition matrix, namely the slightly hydrophobic gas diffusion layer obtained in the fourth step.
Preferably, in the method for modifying a surface of a microporous layer of a gas diffusion layer of a fuel cell described in the fifth step, the electrophoretic deposition dispersion liquid is a mixed solution of cerium salt solution, carbon particles and a hydrophobic agent; the cerium salt is one or more of cerium sulfate and cerium nitrate, the carbon particles are one or more of carbon black, acetylene black, graphene and carbon nanotubes, and the hydrophobic agent is one of PTFE or PVDF.
The method for modifying the surface of the microporous layer of the gas diffusion layer of the fuel cell comprises the following steps of:
Firstly, uniformly mixing electrophoretic deposition dispersion liquid, and placing the mixture in an electrophoretic deposition device;
secondly, placing a stainless steel counter electrode on the positive electrode, placing an electrophoretic deposition matrix on the negative electrode, and completely immersing the positive electrode and the negative electrode in the electrophoretic deposition dispersion liquid;
setting the voltage to be 0-50V for 0-5min;
Finally, taking out the electrophoretic deposition matrix from the dispersion liquid, soaking the electrophoretic deposition matrix in deionized water, removing surface floating liquid, and putting the electrophoretic deposition matrix into a baking oven with the temperature of 50-100 ℃ for baking to obtain the modified microporous layer.
Preferably, the method for modifying the surface of the microporous layer of the gas diffusion layer of the fuel cell in the step six has the sintering temperature of 340-380 ℃, the atmosphere is an air atmosphere, and the sintering time is 20-60 min.
Compared with the prior art, the invention has the beneficial effects that:
According to the application, a layer of nano cerium oxide, a carbon material and a thin layer of a hydrophobic agent are deposited on the surface of a conventional microporous layer, so that a surface modified gas diffusion layer is obtained, HO free radicals generated in the electrochemical reaction process can be effectively captured by the surface modified gas diffusion layer during the operation of a galvanic pile, degradation of a proton exchange membrane caused by free radical attack is prevented, the durability of a fuel cell membrane electrode is improved, and compared with the method of doping cerium oxide directly in microporous layer slurry in the conventional gas diffusion layer, the doped cerium oxide is positioned on the surface layer of the microporous layer and is in direct contact with a catalytic layer, so that the capturing efficiency is greatly improved; in addition, the doping degree of cerium oxide in the microporous layer can be controlled by controlling the thickness of the modified microporous layer, and the structure, thickness and the like of the modified microporous layer can be controlled by adjusting the concentration ratio of each component in the electrophoretic deposition dispersion liquid, the electrochemical current intensity and the deposition time of deposition, and the addition of the modified microporous layer does not change the connection state among carbon particles of the microporous layer, so that the problem of the improvement of the resistivity of the gas diffusion layer caused by cerium oxide doping is solved.
Drawings
Fig. 1 is a schematic view of the structure of a gas diffusion layer in example 2.
Fig. 2 is a schematic view of the structure of the gas diffusion layer in the comparative example.
Detailed Description
The technical scheme of the patent is further described in detail below with reference to the specific embodiments.
Embodiments of the present patent are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present patent and are not to be construed as limiting the present patent.
Example 1
A method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, comprising:
step one: placing a carbon paper substrate in PTFE emulsion with the mass fraction of 10%, standing for 2min, taking out, removing surface floating liquid, drying, placing in a sintering furnace, setting the temperature to 350 ℃, and sintering for 30min to obtain a hydrophobic substrate layer;
Step two: the acetylene black, 10wt.% PTFE emulsion and ethanol are prepared from the following components in percentage by mass: 3:10, fully stirring and mixing the materials in proportion to prepare uniform and stable microporous layer slurry of the gas diffusion layer;
step three: coating the prepared microporous layer slurry on the surface of the hydrophobic treated substrate layer in a knife coating mode, controlling the thickness of a wet film to be 100 mu m, and drying at 100 ℃ to obtain a conventional microporous layer;
step four: presintering at 250deg.C for 20min;
Step five: placing a substrate layer with a conventional microporous layer into an electrophoretic deposition device to serve as a working negative electrode, mixing 200ml of cerium nitrate solution with 0.4g of graphene, 10wt.% of PTFE emulsion and 0.8 g/L of cerium nitrate solution in an electrophoretic deposition dispersion liquid, performing ultrasonic dispersion for 24 hours to obtain a uniform dispersion liquid, setting the voltage to 10V, performing electrophoretic deposition for about 60 seconds to obtain a mixed thin layer of cerium nitrate, graphene and PTFE, taking out, removing surface floating liquid, and drying;
step six: and sintering for 30min in an air atmosphere at 350 ℃ to obtain the modified microporous layer.
Example 2
Referring to fig. 1, a method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, comprising:
Step one: placing a TGP-H-060 carbon paper base material in PTFE emulsion with the concentration of 10wt.% for 2min, taking out, removing surface floating liquid, drying at 100 ℃, and then placing in a sintering furnace at 350 ℃ for sintering for 30min;
Step two: fully stirring and mixing carbon powder, PTFE emulsion and solvent (ethanol and water) to prepare uniform and stable microporous layer slurry of a gas diffusion layer, wherein the solid content of the slurry is 10%, and the PTFE content is 30% of the mass of the carbon powder;
Step three: coating the prepared microporous layer slurry on the surface of the carbon paper substrate subjected to hydrophobic treatment in a knife coating mode, controlling the thickness of a wet film to be 100 mu m, and drying at 100 ℃ for 10min to obtain a conventional microporous layer;
step four: presintering at 250deg.C for 20min;
step five: placing the carbon paper with the conventional microporous layer in cerium nitrate electrolyte with the molar concentration of 0.5mMol, depositing a layer of cerium nitrate on the surface of the conventional microporous layer by an electrodeposition method, controlling the electrochemical voltage to be 5V, depositing for 10s, taking out, cleaning and drying;
step six: and sintering for 30min in an air atmosphere at 350 ℃ to obtain the modified microporous layer.
Comparative example
Referring to fig. 2, a method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, comprising:
Step one: placing a TGP-H-060 carbon paper base material in PTFE emulsion with the concentration of 10wt.% for 2min, taking out, removing surface floating liquid, drying at 100 ℃, and then placing in a sintering furnace at 350 ℃ for sintering for 30min;
Step two: fully stirring and mixing carbon powder, PTFE emulsion and solvent (ethanol and water) to prepare uniform and stable microporous layer slurry of a gas diffusion layer, wherein the solid content of the slurry is 10%, and the PTFE content is 30% of the mass of the carbon powder;
Step three: coating the prepared microporous layer slurry on the surface of the carbon paper substrate subjected to hydrophobic treatment in a knife coating mode, controlling the thickness of a wet film to be 100 mu m, and drying at 100 ℃ for 10min to obtain a conventional microporous layer;
Step four: and then sintering at 340-380 ℃ in an air atmosphere to obtain the conventional gas diffusion layer.
In the fuel cell gas diffusion layer prepared in comparative example 2 and comparative example, a layer of nano cerium oxide particles is deposited on the surface of the microporous layer carbon particles, HO free radicals generated in a reaction can be effectively captured by the surface modified gas diffusion layer during operation of a galvanic pile, degradation of a proton exchange membrane caused by free radical attack is prevented, durability of a fuel cell membrane electrode is improved, and in addition, compared with a method of doping cerium oxide directly in a microporous layer slurry in a conventional gas diffusion layer, the method provided by the application can control the doping degree of cerium oxide in the microporous layer by controlling the thickness of the modified microporous layer, and can also control the size and the number of cerium oxide particles by adjusting the components and concentration ratio of electrolyte, the deposited voltage strength and the deposited time, and the doping of cerium oxide particles does not change the connection state among the microporous layer carbon particles, so that the resistivity of the gas diffusion layer caused by cerium oxide doping is reduced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. A method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell, comprising:
step one: placing the carbon paper substrate in a hydrophobizing agent, taking out, removing surface floating liquid, drying, and then placing in a sintering furnace for sintering to obtain a hydrophobic substrate layer;
step two: preparing uniform and stable microporous layer slurry of the gas diffusion layer by fully stirring and mixing carbon powder, a hydrophobic agent, a solvent and an additive according to a certain proportion;
Step three: coating the prepared microporous layer slurry on the surface of the hydrophobic treated substrate layer in a doctor blade coating, spraying or screen printing mode, and drying to obtain a conventional microporous layer;
Step four: presintering the conventional microporous layer to obtain a gas diffusion layer with stable structure and slight hydrophobicity;
Step five: placing the slightly hydrophobic gas diffusion layer obtained in the step four into an electrophoretic deposition device for electrophoretic deposition, taking out the slightly hydrophobic gas diffusion layer, removing surface floating liquid, and drying to obtain a modified microporous layer;
step six: finally, the surface modified gas diffusion layer is obtained through high-temperature sintering.
2. The method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell according to the step one of claim 1, wherein the substrate layer is carbon fiber paper or carbon fiber cloth, the hydrophobic substrate layer is obtained by soaking a hydrophobizing agent with the mass fraction of 5-15 wt%, drying at 80-120 ℃ and sintering at 340-380 ℃, the solid content of PTFE is controlled to be 5-15% of the mass of the original substrate layer after the hydrophobic treatment, and the hydrophobizing agent is one or more of PTFE and PVDF.
3. The method for surface modification of a microporous layer of a fuel cell gas diffusion layer according to step two of claim 1, wherein the proportion of the microporous layer slurry is generally carbon powder, hydrophobizing agent, solvent, additive = 1:0.1:20:0.01-1:1:5:0.1, the carbon powder is one or more of carbon black, acetylene black and carbon nano tubes, the solvent is one or more of water, ethanol, ethylene glycol, n-propanol and isopropanol, and the additive comprises a pore-forming agent, a dispersing agent, a thickening agent, a leveling agent and the like.
4. The method for surface modification of a microporous layer for a gas diffusion layer for a fuel cell according to step four of claim 1, wherein the presintering temperature of the conventional microporous layer can be set to 180 to 320 ℃ and the presintering time can be set to 10 to 30 minutes.
5. The method for modifying the surface of a microporous layer of a gas diffusion layer of a fuel cell according to step five of claim 1, wherein the electrophoretic deposition device is a two-electrode system device, the anode is a counter electrode, a stainless steel sheet is arranged, and the cathode is an electrophoretic deposition substrate, namely, the slightly hydrophobic gas diffusion layer obtained in step four.
6. The method for modifying the surface of a microporous layer of a gas diffusion layer for a fuel cell according to step five of claim 1, wherein the electrophoretic deposition dispersion liquid is a mixed solution of cerium salt solution, carbon particles, and a hydrophobizing agent; the cerium salt is one or more of cerium sulfate and cerium nitrate, the carbon particles are one or more of carbon black, acetylene black, graphene and carbon nanotubes, and the hydrophobic agent is one of PTFE or PVDF.
7. The method for modifying the surface of a microporous layer of a gas diffusion layer for a fuel cell according to step five of claim 1, wherein the electrophoretic deposition process is specifically:
step one: uniformly mixing the electrophoretic deposition dispersion liquid, and placing the mixture in an electrophoretic deposition device;
Step two: placing a stainless steel counter electrode on the positive electrode, placing an electrophoretic deposition matrix on the negative electrode, and completely immersing the positive electrode and the negative electrode in the electrophoretic deposition dispersion liquid;
step three: setting the voltage to be 0-50V for 0-5min;
Step four: and taking out the electrophoretic deposition matrix from the dispersion liquid, soaking the electrophoretic deposition matrix in deionized water, removing surface floating liquid, and putting the electrophoretic deposition matrix into a baking oven with the temperature of 50-100 ℃ for baking to obtain the modified microporous layer.
8. The method for surface modification of a microporous layer for a gas diffusion layer of a fuel cell according to step six of claim 1, wherein the sintering temperature is 340 to 380 ℃, the atmosphere is an air atmosphere, and the sintering time period is 20 to 60 minutes.
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